Patented May 21, 1935 2 002 105 UNITED STATES PATENT OFFICE PROCESS FOR TREATING VEGETABLE mans Albert 'Bodmer and Ernst Weiss, Wattwll,
Switzerland, assignors to Heberlein Patent Coriorition, New York, N. Y., a corporation of New No Drawing. Application August 10, 1932, serial No. 628,184. In Germany March 17, 1932 8 Claims. (Cl. 8-20) This invention relates to a method of treatis softer; whereas the effect produced by water ing vegetable'fibrous material and to the resultlies intermediate these we effects. ing product. If one employs activated cuprammonium solu- The principal object of the invention is to protion (containing a small quantity of free caustic duce an improved permanent finish f uch aalkali) followed by treatment with alkali, .one 5 terial in a simple efilcient manner. Further obtains half stifi or stifi, as well as linen-like objects and advantages of the invention will more effects, which are fied s 1 661 With fully appear from the following description the efiects secured by the process of the copendwherein certain preferred ways of carrying out ing application mentioned. These eifects accord- 10 the invention are set forth. The inventionwillbe ing to the p es p oces are ur d w 10 more particularly pointed out in the appended decreased ammonia consumption, the copper conclaims. tent remaining unchanged, with the consequence Valuable efiects can be produced on vegetable that the proc i greatly p v r 1Ihe fibers by the action of cuprammonium solution viewpoint f e n my n P fi and caustic alkali solution in accordance with the The novel m od f h pr n invention is 15 procedure of applicants copending application useful for all kinds of vegetable fibrous structures which has now matmed into Patent #1,896,620 as Well as 10058 fi Vegetable fibrous matedated February '7, 1933. That process r t upon rial may be submitted to treatment inthe bleached the production of a swelling effect initially prostate or in any other pre-treated condition as well go duced in a certain manner upon the fibers with as mercerized- Fibrous Structures consisting of a following treatment thereof whereby alteration Vegetable fibers of Various O s 0 mi d w of the properties of the fibrous structure is proother natural or artificial fibers, can be ennobled duced. It has now been discovered in accordinthis manner- By the aid of Suitable apparatus ance with thi inv ti th t very'sman mm. the same*process can be carried out so that by tion of free lk li sharp1yihoreases t swelling the action of the swelling material the fibrous 25 of the material and cessation of swelling structureis not altered throughout, but the swell- (Entquellung) may be arranged so t the ing occurs only on one side and superficially. nobling effect on t fiber is considerably The action not only of the cuprammonium but proved, 1 ha found also in accordance with also of the alkali lye may be carried on while the thi i ti t t t addition and m fibers are ineither loose or tensioned condition. 30 tion of th alk l furthermor permits a very The ennobled fibrous structures, owing to their considerable decrease, to about one-half, of the Plastic Properties, are Very adaptable to $3,553 amount of ammonia requiredin the cuprammoniquent mechanical treatment; for instance by um h tio h addition of alkali must be calendering and the like, extraordinarily supple small so that the amount of free alkali contained (geschmeidige) effects are Prduced- 35 in the solution will not exceed 1.5%. In actual By the novel methd here disclosed, it is also practice it is preferable to work with an amount possible to obtain Patemjng by local action of of free alkali hydroxide of 0.54%. For this h swelling this Purpilse it is purpose caustic soda is employed as alkali alslble employ dn'ect application by Printing 40 though caustic potash and the hydroxides of the spraying or smattering with or without the use 40 of thickeners as well as to use resist printing accompanied by subsequent dipping in to the swell- The cuprammonium solution thus made is ca mg agent In addition, durable patterns can be pable by itself of ennobhng vegetable fibers and produced by subiecting a previously mercenzed to produce efiects of the kind described in the f b to 1 81 h t d th copendin a lication Ser No 321505 0 P t no o pressmg an en su Jec mg 45 g pp i n w a it to the action of swelling agents in accordance out No. 1,896,620 above referred to, whereby as with the present procedure a ul s wha s s e m 1 aus but It has been previously suggested to obtain enatere as y than Obtalnable y the p noblement by the action of cuprammonium soludure of the copending application mentioned, is tion containing a substantial amount of free secured. The discontinuance of swelling of the alkali, always more than 1.5-2% free alkali. fiber according to the kind of effect desired can However, solutions of this kind are not capable be obtained with water, dilute acid or dilute alof producing the ennobling efiects above referred kali lye, whereby generally the efiect produced by to because they cause a noticeable solvent action the dilute alkali is stifier, that with dilute acid on the cellulose subjected to swelling so that the 55 rare earth metals are also useful.
precipitation phenomenon herein described and occurring in the course of the process for eliminating the swelling does not appear. Further the stability of cuprammonium solutions having high alkali content, is limited.
The following are examples of the process employed, these examples being given simply as illustrations. It is to be understood that the invention is not restricted thereto.
Eramples 1. Bleached cretonne fabric of cotton is impreg nated with a cuprammonium solution containing 15 grams of copper and 5 grams of sodium hydroxide per liter and after a short action time of 15 seconds is precipitated by sulfuric acid of 2 B. at 15 C. coincidentally with the acid precipitation the elimination from the fiber of the copper is assured. After calendering the finished fabric exhibits a supple elastic feel resembling linen.
2. Mercerized cotton yarn is briefly treated during 15 seconds with a solution of cuprammonium containing 12 grams of copper and 8 grams of potassium hydroxide per liter and immediately thereafter washed with water at 18 C. Elimination of copper is accomplished in the usual way with dilute acid. The finished yarn resembles linen yarn.
3. Pre-treated calico fabric is passed for a short time through a cuprammonium solution containing 10 grams of copper and 3 grams of sodium hydroxide per liter, after an air passage of 40 seconds, followed by precipitation by the aid of dilute caustic soda at 4 B. at 20 C. Elimination of copper after the latter treatment is effected in the usual manner. Theresult of the ennobling effect is similar to that in Example 1 except that an increased stiffness is noted.
4. Cuprammonium solution .comprising 13 grams of copper and 10 grams of sodium hydroxide per liter is caused to act upon a heavy cotton fabric for 20 seconds at 10 0. Immediately thereafter the swollen unwashed fabric is mercerized in the mercerizing machine with the use of concentrated soda lye, followed by-elimination of copper by acidulation and washing. For finishing intense calendering and mangling are applied with the result that the fabric assumes the characteristics of heavy linens.
5. A resist-printed fabric is treated according to the procedure in Example 4. The fabric exhibits patterning of damask-like nature; the reserve portions of the fabric show unaltered properties, and thus contrast with the other parts that have been subjected to the action of cuprammonium solution.
6. Card sliver made of ramie fibers is impregnated with a, solution of cuprammonium containing .14 grams of copper and 4 grams of sodium hydroxide per liter and after a reaction time of 30 seconds then subjected to mercerizing with. soda lye and is de-coppered in the usual manner. After drying there results a lustrous stifi fiber of agglutinated ramie fibers or filaments.
Thus while we have described our improvements in detail and with respect to certain preferred forms, we do not desire to be limited to such details or forms since, as will be understood by those skilled in the art-after understanding our inv ntion, many changes and modifications may be made and the invention embodied in widely different forms without departing from the spirit and scope thereof in its broader aspects, and we desire to cover all modifications, forms and embodiments coming within the scope of any one or more of the appended claims.
Having thus described our invention, what we claim as new and desire to secure by Letters Patent, is:-
1. A method of producing permanent finish effects on vegetable cellulose material which comprises preparing a bath containing cuprammonium and a free alkali metal hydroxide in which the percentage of free alkali does not exceed 1.5%
of the weight of the solution, swelling the vegetable cellulose material by subjecting it to the bath and subjecting the so-treated material to an agent for interrupting the swelling action of said solution.
2. The method according to claim 1 in which the amount of free alkali is from 0.5 to 1%.
3. The method according to claim 1 in which the interruption of the swelling is efiected by dilute acid.
4. The method according to claim 1 in which the swelling is interrupted by treatment with water.
5. The method according to claim 1 in which the swelling is interrupted by treatment with dilute alkali lye.
6. The method according to claim 1 in which the interruption of swelling is effected by treating the fibrous materials after treatment with the alkaline cuprammonium solution with concentrated alkali lye of a strength to cause mercerization thereof.
/ 7. The method according to claim 1 in which the alkaline cuprammonium solution acts on the material to form a pattern.
8. Steps in the method of producing permanent finish efiects on vegetable cellulose material which consist in preparing a cuprammonium solution containing a free alkali metal hydroxide in which the percentage of free alkali does not exceed 1.5% of the weight of the solution, and subjecting the vegetable cellulose material to said solution.
ALBERT BODMER. ERNST WEISS.